# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 1145/167 #============================================================================ data_global #============================================================================ _audit_creation_method 'form.cif (version 2.0)' # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Prof.Fun Hoong Kun' _publ_contact_author_address ; X-ray Crystallography Unit School of Physics Universiti Sains Malaysia 11800 USM, Penang MALAYSIA ; _publ_contact_author_email 'hkfun@usm.my' _publ_contact_author_fax '6 04 6579150' _publ_contact_author_phone '6 04 6577888 Ext. 3690' _publ_requested_journal 'Acta Crystallographica C' _publ_requested_category 'FO' _publ_requested_coeditor_name 'Prof A.J.Blake' _publ_contact_letter ; Date : January 1998 The Managing Editor International Union of Crystallography 5 Abbey Square Chester CH1 2HU England Ref: Paper submitted to Acta Cryst 'C'. Dear Sir, Attached is a manuscript with the after-mentioned title and authors which I wish to submit for publication in Acta Cryst. C. The structure factor tables and the figure shall be emailed to you after receiving the reference number. The letter of submission, the transfer of copyright form and the chemical diagram shall be sent in hard copy forms to you subsequently. Yours Sincerely, Hoong-Kun Fun ; #============================================================================ # TITLE AND AUTHOR LIST _publ_section_title ; ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Hoong-Kun Fun' ? ; X-ray Crystallography Unit School of Physics Universiti Sains Malaysia 11800 USM, Penang Malaysia ; 'Kandasamy Chinnakali' ; On leave from: Department of Physics Anna University, Chennai(Madras)-600025, India ; ; X-ray Crystallography Unit School of Physics Universiti Sains Malaysia 11800 USM, Penang Malaysia ; #============================================================================ # TEXT _publ_section_abstract ; ; _publ_section_comment ; Scheme I ; _publ_section_acknowledgements ; The authors would like to thank the Malaysian Government and Universiti Sains Malaysia for research grant R&D No. 190-9609-2801. KC thanks the Universiti Sains Malaysia for a Visiting Post Doctoral Fellowship. ; _publ_section_references ; Nardelli, M. (1983). Acta Cryst. C39, 1141-1142. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption correction of Area Dectector Data, Univ. of Gottingen, Germany. Siemens (1996). SAINT v4 Software Reference Manual, Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Siemens (1996). SHELXTL Version 5 Reference Manual, Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Siemens (1996). SMART Software Reference Manual, Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. ; _publ_section_figure_captions ; Fig.1. The structure of title compound showing 50% probability displacement ellipsoids and the atom-numbering scheme. ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; The data collection was covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 30s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating thirty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. The structure was solved by direct methods and refined by full-matrix least-squares techniques. All H-atoms were located from a difference Fourier map and refined isotropically. ; #============================================================================ data_bjf3m _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H20 Ni S8' _chemical_formula_weight 527.51 _chemical_melting_point ? _chemical_compound_source ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.171(2) _cell_length_b 5.2299(7) _cell_length_c 16.567(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.709(10) _cell_angle_gamma 90.00 _cell_volume 1004.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4085 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 33.0 _exptl_crystal_description plate _exptl_crystal_colour 'bluish black' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method ? _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 1.796 _exptl_absorpt_correction_type 'empirical using SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.633 _exptl_absorpt_correction_T_max 0.789 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5078 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0194 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 24.74 _reflns_number_total 1706 _reflns_number_observed 1563 _reflns_observed_criterion >2sigma(I) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Sheldrick, 1996)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1996)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1996)' _computing_publication_material ; SHELXTL (Sheldrick, 1996) PARST (Nardelli, 1995) ; _refine_special_details ; Refinement on F^2^ for ALL reflections. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating observed R-factor etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.4578P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1706 _refine_ls_number_parameters 155 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_obs 0.0211 _refine_ls_wR_factor_all 0.0528 _refine_ls_wR_factor_obs 0.0510 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.074 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni Ni 0.0000 0.0000 0.0000 0.03121(12) Uani 1 d S . S1 S 0.16183(4) 0.04080(10) -0.02353(3) 0.03639(14) Uani 1 d . . S2 S 0.06995(4) -0.27240(11) 0.09734(3) 0.03795(15) Uani 1 d . . S3 S 0.39071(4) -0.17323(11) 0.03652(3) 0.03754(15) Uani 1 d . . S4 S 0.28650(4) -0.54153(10) 0.17094(4) 0.03713(14) Uani 1 d . . C1 C 0.2512(2) -0.1705(4) 0.04416(12) 0.0279(4) Uani 1 d . . C2 C 0.2101(2) -0.3119(3) 0.09975(12) 0.0287(4) Uani 1 d . . C3 C 0.4696(2) -0.4197(4) 0.11014(12) 0.0297(4) Uani 1 d . . C4 C 0.4351(2) -0.4387(4) 0.19064(12) 0.0284(4) Uani 1 d . . C5 C 0.4649(2) -0.2012(4) 0.24604(13) 0.0343(5) Uani 1 d . . C6 C 0.5933(2) -0.1387(5) 0.26683(15) 0.0407(5) Uani 1 d . . C7 C 0.6307(2) -0.1164(4) 0.18779(15) 0.0396(5) Uani 1 d . . C8 C 0.5979(2) -0.3505(4) 0.13095(14) 0.0342(4) Uani 1 d . . H3 H 0.4548(17) -0.5783(41) 0.0823(13) 0.031(5) Uiso 1 d . . H4 H 0.4763(17) -0.5828(38) 0.2220(13) 0.029(5) Uiso 1 d . . H5A H 0.4177(18) -0.0545(40) 0.2159(13) 0.034(5) Uiso 1 d . . H5B H 0.4465(18) -0.2289(40) 0.2965(15) 0.037(6) Uiso 1 d . . H6A H 0.6095(21) 0.0144(45) 0.2989(16) 0.048(7) Uiso 1 d . . H6B H 0.6350(20) -0.2644(44) 0.2988(14) 0.038(6) Uiso 1 d . . H7A H 0.7136(20) -0.0966(42) 0.2001(14) 0.042(6) Uiso 1 d . . H7B H 0.5964(19) 0.0347(44) 0.1561(15) 0.044(7) Uiso 1 d . . H8B H 0.6171(18) -0.3308(41) 0.0798(14) 0.039(6) Uiso 1 d . . H8A H 0.6384(21) -0.5006(44) 0.1591(15) 0.045(6) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0235(2) 0.0403(2) 0.0281(2) 0.00740(15) 0.00515(14) 0.00489(14) S1 0.0278(3) 0.0478(3) 0.0328(3) 0.0141(2) 0.0081(2) 0.0060(2) S2 0.0258(3) 0.0490(3) 0.0391(3) 0.0167(2) 0.0100(2) 0.0055(2) S3 0.0267(3) 0.0508(3) 0.0361(3) 0.0136(2) 0.0110(2) 0.0065(2) S4 0.0280(3) 0.0340(3) 0.0467(3) 0.0151(2) 0.0073(2) 0.0008(2) C1 0.0247(9) 0.0324(10) 0.0247(9) -0.0011(8) 0.0049(7) 0.0011(8) C2 0.0254(9) 0.0286(10) 0.0293(10) 0.0016(8) 0.0045(8) 0.0015(8) C3 0.0277(10) 0.0275(10) 0.0316(10) -0.0026(8) 0.0057(8) 0.0044(8) C4 0.0255(10) 0.0251(9) 0.0322(10) 0.0037(8) 0.0053(8) 0.0046(8) C5 0.0359(11) 0.0347(11) 0.0318(11) -0.0034(9) 0.0094(9) 0.0036(9) C6 0.0366(12) 0.0408(12) 0.0387(12) -0.0102(10) 0.0027(10) -0.0021(10) C7 0.0284(11) 0.0419(12) 0.0443(12) -0.0004(10) 0.0049(9) -0.0058(9) C8 0.0274(10) 0.0393(12) 0.0359(11) 0.0008(9) 0.0095(9) 0.0053(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S2 2.1260(5) . ? Ni S2 2.1260(5) 3 ? Ni S1 2.1317(6) 3 ? Ni S1 2.1317(6) . ? S1 C1 1.709(2) . ? S2 C2 1.707(2) . ? S3 C1 1.740(2) . ? S3 C3 1.833(2) . ? S4 C2 1.741(2) . ? S4 C4 1.819(2) . ? C1 C2 1.388(3) . ? C3 C4 1.518(3) . ? C3 C8 1.535(3) . ? C4 C5 1.521(3) . ? C5 C6 1.529(3) . ? C6 C7 1.516(3) . ? C7 C8 1.522(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni S2 180.0 . 3 ? S2 Ni S1 88.47(2) . 3 ? S2 Ni S1 91.53(2) 3 3 ? S2 Ni S1 91.53(2) . . ? S2 Ni S1 88.47(2) 3 . ? S1 Ni S1 180.0 3 . ? C1 S1 Ni 104.75(7) . . ? C2 S2 Ni 105.40(7) . . ? C1 S3 C3 106.43(9) . . ? C2 S4 C4 102.39(9) . . ? C2 C1 S1 119.59(14) . . ? C2 C1 S3 126.91(15) . . ? S1 C1 S3 113.46(11) . . ? C1 C2 S2 118.67(14) . . ? C1 C2 S4 126.23(15) . . ? S2 C2 S4 115.04(11) . . ? C4 C3 C8 110.6(2) . . ? C4 C3 S3 113.66(13) . . ? C8 C3 S3 105.95(14) . . ? C3 C4 C5 113.4(2) . . ? C3 C4 S4 112.78(13) . . ? C5 C4 S4 113.04(13) . . ? C4 C5 C6 110.5(2) . . ? C7 C6 C5 112.1(2) . . ? C6 C7 C8 112.4(2) . . ? C7 C8 C3 112.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ni S1 C1 2.16(7) . . . . ? S2 Ni S1 C1 -177.84(7) 3 . . . ? S1 Ni S1 C1 -31.9(1000) 3 . . . ? S2 Ni S2 C2 103.0(558) 3 . . . ? S1 Ni S2 C2 178.21(7) 3 . . . ? S1 Ni S2 C2 -1.79(7) . . . . ? Ni S1 C1 C2 -2.3(2) . . . . ? Ni S1 C1 S3 179.83(8) . . . . ? C3 S3 C1 C2 4.7(2) . . . . ? C3 S3 C1 S1 -177.57(10) . . . . ? S1 C1 C2 S2 0.9(2) . . . . ? S3 C1 C2 S2 178.55(11) . . . . ? S1 C1 C2 S4 178.08(11) . . . . ? S3 C1 C2 S4 -4.3(3) . . . . ? Ni S2 C2 C1 0.9(2) . . . . ? Ni S2 C2 S4 -176.55(8) . . . . ? C4 S4 C2 C1 26.5(2) . . . . ? C4 S4 C2 S2 -156.25(11) . . . . ? C1 S3 C3 C4 -35.7(2) . . . . ? C1 S3 C3 C8 -157.36(13) . . . . ? C8 C3 C4 C5 53.8(2) . . . . ? S3 C3 C4 C5 -65.2(2) . . . . ? C8 C3 C4 S4 -176.07(13) . . . . ? S3 C3 C4 S4 64.9(2) . . . . ? C2 S4 C4 C3 -57.06(15) . . . . ? C2 S4 C4 C5 73.3(2) . . . . ? C3 C4 C5 C6 -55.1(2) . . . . ? S4 C4 C5 C6 174.90(15) . . . . ? C4 C5 C6 C7 53.9(3) . . . . ? C5 C6 C7 C8 -53.2(3) . . . . ? C6 C7 C8 C3 52.1(2) . . . . ? C4 C3 C8 C7 -51.6(2) . . . . ? S3 C3 C8 C7 72.0(2) . . . . ? _refine_diff_density_max 0.300 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.045 #============================================================================ # END OF CIF